WO2010107340A1 - Matériau d'anode pour source d'énergie chimiques et procédé de fabrication correspondant - Google Patents

Matériau d'anode pour source d'énergie chimiques et procédé de fabrication correspondant Download PDF

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Publication number
WO2010107340A1
WO2010107340A1 PCT/RU2010/000086 RU2010000086W WO2010107340A1 WO 2010107340 A1 WO2010107340 A1 WO 2010107340A1 RU 2010000086 W RU2010000086 W RU 2010000086W WO 2010107340 A1 WO2010107340 A1 WO 2010107340A1
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Prior art keywords
lithium
stage
temperature
anode material
mixture
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PCT/RU2010/000086
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English (en)
Russian (ru)
Inventor
Вадим Сергеевич ГОРШКОВ
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Общество С Ограниченной Ответственностью "Элионт"
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Priority to EP10753758.1A priority Critical patent/EP2405512B1/fr
Priority to CN201080019545.7A priority patent/CN102714309B/zh
Publication of WO2010107340A1 publication Critical patent/WO2010107340A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G37/00—Compounds of chromium
    • C01G37/006—Compounds containing, besides chromium, two or more other elements, with the exception of oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to the electrical industry, in particular, to anode materials for chemical current sources (CIT) and can be used as starting material for lithium-ion secondary batteries (accumulators) intended for applications requiring high capacity and high working currents, for example, for electric vehicles - HEV (hybrid electric car), PHEV (rechargeable hybrid electric car), BEV (battery electric car), or a portable electric tool.
  • CIT chemical current sources
  • accumulators lithium-ion secondary batteries
  • the level of technology Currently, the most used pair of electrodes in lithium-ion batteries is a pair of LiCoO 2 / C (carbon). However, the compound LiC 6 , which is formed when lithium ions are introduced into the carbon structure, for example, graphite, is explosive.
  • This formula expresses the formation of two nonequivalent sublattices with octahedral positions of the 16c and lbd types. Since in the described process the initial tetrahedral sites, when filled with additional lithium atoms, become octahedral (8a ⁇ 16c), this concentration phase transition is possible only if all tetrahedral positions in the initial spinel structure are occupied by mobile lithium.
  • the charged form of the material - Li 7 Ti 5 Oj 2 is completely safe, unlike LiC 6 and, especially, metallic lithium,
  • titanium has a high oxidation state of 4+, and the charge balance can be expressed by the formula Li + 4 Ti 4+ 5 0 2 ⁇ i 2 . Since titanium ion 4+ has an electronic configuration of ⁇ d °, the valence band is completely filled, and the conduction band
  • the electronic conductivity, as for other dielectrics, is determined by the “imperfections” of the sample, primarily the presence and concentration of impurities giving donor and acceptor levels, as well as intrinsic defectiveness. According to many published sources, the electronic conductivity of Li 4 Ti 5 Oi 2 under normal conditions lies in the range 100 10 ⁇ 8 - 10 ⁇ 13 ohm "1- cm " 1 . [FROM. H. Schep, JT Vaugeu, AN Japsep, DW Dees, AJ Kahaiap, T. Goascher, MM Thasker.
  • compositions with electrically conductive polymers have also been proposed.
  • the electrode material is an electrically conductive additive.
  • Li 7 Ti 5 O 12 phase obtained from the starting material upon its discharge is a very good conductor, since it contains a high concentration of Ti 3+ ( ⁇ d 1 ), i.e. electrons in the conduction band (in accordance with the formula Li 7 Ti 3+ zTi 4+ 2 ⁇ j 2 ).
  • Li 4 Ti 5 Oi 2 particles (starting from the composition L locker + ⁇ is ⁇ i ⁇ , where ⁇ ⁇ 0.1, i.e. ⁇ 1/30 of the total capacity) are covered with a conductive layer of Li 7 Ti S O 12 which makes the presence of a previously created layer redundant. Further, the process proceeds along the interphase boundary between Li 4 Ti 5 O 12 and Li 7 Ti 5 Oi 2 , i.e. lithium ions and electrons enter the reaction zone through the layer
  • the concentration of the alloying element is such that the type of crystalline structure of the starting material does not change. As a result of such substitution, impurity charge defects are formed in the substance, which serve as carriers of electric current.
  • the known method is a prototype of the receipt of the specified anode material for
  • lithium-ion HIT includes the preparation of a mixture of the starting components containing lithium and titanium by homogenization and grinding, followed by heat treatment of the prepared mixture in a controlled atmosphere from inert and reducing gases. Moreover, hydrogen, hydrocarbons, carbon monoxide are used as reducing gases, and the reduction process (heat treatment)
  • the objective of the present invention is to obtain an anode material for lithium-ion ChIT having high electrical conductivity and electrochemical 260 capacity for use in devices operating at high discharge currents.
  • the problem is solved in that the known anode material for lithium-ionic chitos based on lithium-titanium spinel of the chemical formula Li 4 Ti 5 0i 2-x , where x is the deviation from stoichiometry in the range 0 ⁇ x ⁇ 0.02,
  • ACCORDING TO THE INVENTION contains alloying components — chromium and vanadium in equivalent amounts to achieve the composition of the formula Li 4 Ti 5 . 2 y (Cr y V y ) O 12-x , where 0.02 ⁇ x ⁇ 0.5, y is the stoichiometric coefficient in the range 0 ⁇ y ⁇ 0.25.
  • anode material for lithium-ionic chitosan comprising preparing a mixture of starting components containing lithium and titanium, by homogenization and grinding, followed by heat treatment of the prepared mixture in an atmosphere of inert and reducing gases, ACCORDING TO THE INVENTION, sources of alloying elements — chromium and vanadium — are introduced into the mixture of the starting components, grinding 275 is carried out to obtain particles with a size of no more than 0.5 microns, and heat treatment is carried out step by step in an atmosphere of argon and acetylene, adjusting the volume ratio of gases in the argon: acetylene stream from 999: 1 to 750: 250, respectively, according to the following scheme:
  • the mixture of components is heated to a temperature not exceeding 350 ° C;
  • heating is continued in the temperature range 350 - 750 ° C with a speed of not more than 10 ° C / min, providing solid-phase interaction of the components;
  • the temperature is increased to 840 - 850 0 C and the resulting product is held at this temperature for at least 1 hour;
  • the temperature is lowered to 520 - 580 ° C with a speed of no more
  • the finished anode material is purged with pure argon 290 when cooled to 40 - 60 ° C and packaged.
  • the type of alloying elements and their concentration are selected in such a way that these elements appear only at the octahedral positions of the crystal structure, which ensures the cyclicality of the material in the electrochemical process; 00 - grinding of the starting components to obtain particles no larger than
  • the temperature, speed and time regimes of stepwise heat treatment contribute to the main reaction in the solid phase without melting, without a significant increase in the particle size of the material, without the formation of impurity compounds and low-reaction titanium oxide in the form of rutile, with the achievement
  • the final heat treatment step when purging with pure argon prevents oxidation of the finished anode material during cooling, protecting it also from moisture absorption from the atmosphere.
  • Electrochemical potential 1.53 ⁇ 0.01 V 320 The best embodiment of the invention.
  • the best option has been selected from a large-scale series of experiments (more than 100) for the production of anode material for lithium-ion chemically active compounds carried out in laboratory conditions of an electrochemical plant in the Ural region.
  • the starting components were homogenized (mixed) and placed in a ball mill for grinding to a particle size of not more than 0.5 ⁇ m.
  • the degree of homogeneity of the mixture was characterized by the fact that an arbitrary sample of a mixture of reagents weighing not more than 0.1 g contained an excess of any of the components not more than 0.1%.
  • 360 the prepared mixture of components was placed in a tube furnace with a controlled gas atmosphere, creating a volumetric ratio of gases in the argon: acetylene stream, respectively 750: 250.
  • the heat treatment was carried out in stages according to the following scheme:
  • the mixture of components was heated to a temperature of 350 ° C;
  • heating was continued in the temperature range 350 - 750 ° C with a speed of 10 ° C / min, providing solid-phase interaction (recovery) of the components according to the main reaction;
  • the temperature was increased to 850 ° C and the resulting product was held at this temperature for 1 hour;
  • the temperature was lowered to 550 ° C at a rate of 4 ° C / min and the obtained anode material was kept at this temperature for 2 hours; - at the finish stage, the finished anode material was purged with pure argon while cooling to a temperature below 50 0 C and packed in containers in
  • the inventive anode material for lithium-ion ChIT having high electrochemical capacity (165 ⁇ 5 mA-h / g) and electronic conductivity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

La présente invention concerne l'industrie électrotechnique, et plus précisément des matériaux anodiques pour les cellules électrochimiques aux ions de lithium. Elle porte sur un matériau d'anode pour cellules électrochimiques, qui est basé sur le spinelle lithium-titane et correspond à la formule chimique Li(4)Ti(5-2y) ((Cr(y)V(y)) O(12-x), où « x » est un écart par rapport à la stoechiométrie de l'ordre de 0,02 <x <0,05, et « y » est le coefficient stoechiométrique de l'ordre de 0 <y <0,25. Le procédé de fabrication du matériau d'anode consiste à préparer un mélange de composants de départ, qui contiennent du lithium et du titane et des sources d'alliages de chrome et de vanadium, par l'homogénéisation et le broyage, effectués jusqu'à ce que les particules aient une taille inférieure ou égale à 0,5 micromètres, après quoi on effectue un traitement thermique du mélange étape par étape dans une atmosphère contrôlée constituée d'argon inerte, puis on effectue la préparation du mélange d'acétylène de réduction avec de l'argon, avec un rapport de gaz dans le flux de 999:1 à 750:250, respectivement, en utilisant le schéma suivant: dans un premier stade, le mélange des composants est chauffé à une température ne dépassant pas 350 ° C, dans un deuxième stade, on poursuit le réchauffement dans une plage de températures de 350-750 ° C. Dans un troisième stade, la température est portée à 840-880°C; dans un quatrième stade, la température est abaissée à 520-580 °C. Au stade final, l'argon pur est soufflé sur le matériau d'anode fini lors du refroidissement à 40-60 ° C, puis ce matériau est mis sous emballage. L'invention permet d'augmenter la capacité électrochimique et la conductivité électronique.
PCT/RU2010/000086 2009-03-06 2010-02-25 Matériau d'anode pour source d'énergie chimiques et procédé de fabrication correspondant WO2010107340A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP10753758.1A EP2405512B1 (fr) 2009-03-06 2010-02-25 Matériau d'anode pour sources d'énergie chimique et procédé de fabrication correspondant
CN201080019545.7A CN102714309B (zh) 2009-03-06 2010-02-25 用于电化学电池的阳极材料及其制造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2009107944/09A RU2397576C1 (ru) 2009-03-06 2009-03-06 Анодный материал для литий-ионных хит и способ его получения
RU2009107944 2009-03-06

Publications (1)

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WO2010107340A1 true WO2010107340A1 (fr) 2010-09-23

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US (2) US8367249B2 (fr)
EP (1) EP2405512B1 (fr)
KR (1) KR20120004987A (fr)
CN (1) CN102714309B (fr)
RU (1) RU2397576C1 (fr)
WO (1) WO2010107340A1 (fr)

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CN102844912B (zh) * 2011-02-15 2016-07-13 松下知识产权经营株式会社 锂离子二次电池用负极活性物质材料及其制造方法
RU2495752C1 (ru) * 2012-04-02 2013-10-20 Федеральное государственное бюджетное учреждение науки Институт неорганической химии им. А.В. Николаева Сибирского отделения Российской академии наук (ИНХ СО РАН) Способ получения композиционного материала, содержащего слоистые материалы на основе графита и сульфида молибдена
KR101708361B1 (ko) 2012-08-21 2017-02-20 삼성에스디아이 주식회사 복합 음극 활물질, 그 제조방법, 및 이를 포함하는 리튬 전지
KR20140025160A (ko) 2012-08-21 2014-03-04 삼성에스디아이 주식회사 복합 음극 활물질, 그 제조방법, 및 이를 포함하는 리튬 전지
GB2508218A (en) * 2012-11-26 2014-05-28 Leclanch S A Electrode for the reduction of gassing in lithium titanate cells
EP3709402A1 (fr) * 2014-09-10 2020-09-16 Kabushiki Kaisha Toshiba Batterie électrolytique non aqueuse
EP3353844B1 (fr) 2015-03-27 2022-05-11 Mason K. Harrup Solvants entièrement inorganiques pour électrolytes
US10707531B1 (en) 2016-09-27 2020-07-07 New Dominion Enterprises Inc. All-inorganic solvents for electrolytes
CN110459750B (zh) * 2019-08-21 2023-06-09 内蒙古骅扬高新材料科技有限公司 一种锂离子动力电池负极材料及其制备方法
CN112456546A (zh) * 2020-12-09 2021-03-09 昆明理工大学 一种锂离子电池电极材料及其制备方法

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See also references of EP2405512A4 *
T. OHZUKU, A. UEDA, N. YAMAMOTO.: "Zero-Strain Insertion Material of Li[Li1/3Ti5/3]O4 for Rechargeable Lithium Cells", J. ELECTROCHEM. SOC., vol. 142. - 1, 1995, pages 1431 - 1435, XP002401881, DOI: doi:10.1149/1.2048592
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Z. ZHONG.: "Synthesis of Mo4+ Substituted Spinel Li4Tis-xMoxOlz", ELECTROCHEMICAL AND SOLID-STATE LETTERS, vol. 10, no. 12, 2007, pages A267 - A269

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KR20120004987A (ko) 2012-01-13
CN102714309A (zh) 2012-10-03
EP2405512A1 (fr) 2012-01-11
US8475960B2 (en) 2013-07-02
RU2397576C1 (ru) 2010-08-20
EP2405512A4 (fr) 2013-09-04
US20100224824A1 (en) 2010-09-09
US8367249B2 (en) 2013-02-05
CN102714309B (zh) 2015-02-18
EP2405512B1 (fr) 2014-08-20
US20130048923A1 (en) 2013-02-28

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